l-[3-13C] Phenylalanine and l-[3-13C] tyrosine were synthesized.[α-13C] Benzyl bromides were prepared from [13C] carbon monoxide via the palladium-catalyzed carboalkoxylation of aryl halides. The asymmetric carbon corresponding to the 2-position in phenylalanine was introduced by the diastereoselective alkylation of Dellaria's oxazinone with [α-13C] benzyl bromides. Finally, ethanolysis, deprotection, hydrogenolysis and acid hydrolysis of the ...